Carbohydrate Polymers 136 (2016) 107112

Contents lists available at ScienceDirect

Carbohydrate Polymers
journal homepage: www.elsevier.com/locate/carbpol

Properties of baked foams from citric acid modied cassava starch

and native cassava starch blends
Kanlaya Pornsuksomboon a , Berta Barta Holl b , Katalin Mszros Szcsnyi b ,
Kaewta Kaewtatip a,
a
b

Department of Materials Science and Technology, Faculty of Science, Prince of Songkla University, Hat Yai, Songkhla 90112, Thailand
Department of Chemistry, Biochemistry and Environmental Protection, University of Novi Sad, Novi Sad 21000, Serbia

a r t i c l e

i n f o

Article history:
Received 22 May 2015
Received in revised form 21 August 2015
Accepted 7 September 2015
Available online 9 September 2015
Keywords:
Foam
Starch
Citric acid
Thermal stability
Density

a b s t r a c t
Starch foams from native cassava starch (NS) and citric acid modied cassava starch (CNS) were prepared
using baking processes with blend ratios of 80/20, 60/40, 50/50, 40/60 and 20/80. The density, thickness,
morphology, thermal stability and water absorption of the NS, CNS and blended starch foams were determined. The ratio of the two starch components had a signicant inuence on the density and thickness of
the blended starch foams. All blended starch foams showed good water resistance. Moreover, the morphology of the blended starch foam with the NS/CNS ratio of 50/50 showed a more ordered distribution
of cell sizes with thicker cell walls than for the NS and CNS foams. The thermal stability of the blended
starch foams was somewhat lower than the stability of the NS foam but not to the extent that it affected
any potential practical applications.
2015 Elsevier Ltd. All rights reserved.

1. Introduction
Petroleum-based foams are widely used for packaging, storage
and transportation, automobile industry or as thermal insulation
materials due to their low production costs, light weight, high
modulus, excellent dimensional stability and thermal insulation
(Kaemmerlen, Asllanaj, Jeandel, & Baillis, 2010; Xing et al., 2013).
However, petroleum-based foam is not biodegradable, is difcult
to recycle (Ojeda et al., 2009; Pushpadass, Weber, Dumais, & Hanna,
2010) and may generate toxic decomposition products (Gao, Zheng,
Zhou, Hu, & Feng, 2015). If used as food wrappers, toxic chemicals
released from petroleum-based foam may contaminate the food.
Recently, research and development on starch foams has become
attractive to try to nd substitutes to replace petroleum-based
foams that cause worldwide environmental problems. Starch is
one of the renewable materials that provides several advantages,
such as, it is an abundant resource, is low cost as well as having
good biodegradability (Kaisangsri, Kerdchoechuen, & Laohakunjit,
2012; Pornsuksomboon, Szecsenyi, Hollo, & Kaewtatip, 2014; Silva,
Nievola, Tischer, Mali, & Faria-Tischer, 2013). The process for production of starch foams is simple as they can be prepared using
water as the blowing agent and baking the foam. As a consequence,

Corresponding author.
E-mail address: kaewta.k@psu.ac.th (K. Kaewtatip).
http://dx.doi.org/10.1016/j.carbpol.2015.09.019
0144-8617/ 2015 Elsevier Ltd. All rights reserved.

the production is fast and convenient because it takes place in only

one step. In addition, the production cost is low (Lopez-Gil, SilvaBellucci, Velasco, Ardanuy, & Rodriguez-Perez, 2015). However,
the starch foams made from native starch have some limitations
including their poor mechanical properties, fragility and high water
absorption capability (Kaisangsri et al., 2012; Lee, Chen, & Hannaj,
2008; Pornsuksomboon et al., 2014). These drawbacks need to be
signicantly reduced in order to improve their quality and perhaps also broaden the application areas for starch foams instead of
petroleum-based materials. Starch foams prepared from modied
starch such as acetylated starch, hydroxypropylated starch, cationic
starch, distarch phosphate and glyoxal cross-linking starch exhibit
better mechanical properties with a higher water resistance than
that of starch foam made from native starch (Kaewtatip, Poungroi,
Hollo, & Szecsenyi, 2014; Pornsuksomboon et al., 2014; Uslu &
Polat, 2012; Xu & Hanna, 2005). There are many reagents available
for the modication of starch, for example, glutaraldehyde, boric
acid, glyoxal and epichlorohydrin. However, some of these agents
are toxic and not cost-effective (Ghanbarzadeh, Almasi, & Entezami,
2011). Citric acid (CA) is an inexpensive chemical, which is considered to be harmless in comparison to other substances used
for the derivatization of starch (Ma, Chang, Yu, & Stumborg, 2009;
Wilpiszewska & Czech, 2014). Ma et al. (2009) observed that citric
acid modied starch was a granular resistant starch. Ghanbarzadeh
et al. (2011) reported that citric acid may be used as a cross-linking
agent. The three carboxyl groups of citric acid react with the starch

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K. Pornsuksomboon et al. / Carbohydrate Polymers 136 (2016) 107112

hydroxyl groups to produce esters. In addition, the hydrogen bonding capability of this modied starch derivative increased, thus
hindering its recrystallization and retrogradation. In recent years,
several studies have reported on the use of citric acid modied
starch as a reinforcement ller in starch-based biocomposites in
order to obtain compatible and high performance composite materials. However, to our knowledge, there have been no studies about
the preparation and characterization of starch foams using citric
acid modied starch.
The objectives of this work were to prepare citric acid modied
cassava starch (CNS) and starch foams using native cassava starch
(NS), CNS and blends of CNS and NS with ratios of 80/20, 60/40,
50/50, 40/60 and 20/80. The formation of the CNS was supported by
Fourier transform infrared spectroscopy (FT-IR) while the morphology of the samples was evaluated on the basis of scanning electron
microscopy (SEM). Furthermore, the density, the morphology, the
water adsorption and the thermal properties of NS, CNS and the
blended starch foams were compared and discussed.
2. Experimental
2.1. Materials
Native cassava starch (NS, PD 10369) was kindly supplied by
Siam Modied Starch Co., Ltd. Starch was dried at 105 C for 48 h in
an oven and kept in a desiccator prior to use. Citric acid and glycerol
were from RCI Labscan and Ajax Finechem, respectively. Guar gum
and magnesium stearate were from SigmaAldrich, Inc.
2.2. Citric acid modied cassava starch (CNS) preparation
The citric acid modied cassava starch was prepared by the procedure described by Ma et al. (2009). About 40 g (0.21 mol) of citric
acid was dissolved in 100 ml distilled water. The pH of the solution was then adjusted to pH 4 by adding 22 ml of 10 M NaOH
(0.22 mol). This mixture was combined with 100 g of dried cassava
starch and stirred to obtain an homogeneous slurry. The slurry was
stored for 12 h at room temperature and dried at 80 C for 15 h.
The dried sample was washed 34 times with distilled water to
ensure the complete removal of the unreacted citric acid and NaOH.
Finally, the precipitate was ground in a mortar grinder and dried in
an oven at 105 C until constant weight was achieved and kept in a
desiccator until used.
2.3. Foam preparation
The starch foams were prepared according to previously
described procedure (Kaewtatip et al., 2014) by blending native
cassava starch and citric acid modied cassava starch granules with
ratios of 100/0, 80/20, 60/40, 50/50, 40/60, 20/80 and 0/100. The
total amount of the blending mixtures of NS and CNS was 200 g. The
guar gum and magnesium stearate content was 1 g and 2 g, respectively. The components were mixed at room temperature for 10 min
using a Kenwood KM 262 mixer. Glycerol (5 g) and distilled water
(100 g) were added to the mixture. The batter was further mixed for
10 min and thermo-molded (15 cm 15 cm 4 mm) using a compression molding machine (KT-7014 produced by Kao Tieh Ltd.
(Taipei, Taiwan)) operating at 180 C under a pressure of 1000 psi
for 5 min.
2.4. Characterization
The density was calculated as the relationship between weight
and volume. Sample pieces were stored at 55% RH and 25 C for 7
days before testing. Ten specimens were tested for every sample.

Fig. 1. FTIR spectra of native cassava starch granules (NS), citric acid modied cassava starch granules (CNS) and citric acid (CA).

The thickness was measured with a vernier digital (Kovet ,

Thailand). Sample pieces were stored at 55% RH and 25 C for 7
days before testing. Ten specimens were tested for every sample.
The FT-IR spectra were recorded on a Bruker Tensor 27 Fourier
transform infrared spectrometer using KBr pellets in the frequency
range of 4000400 cm1 . Samples were dried in an oven at 105 C
for 24 h before testing. For each spectrum 512 consecutive scans
were recorded with a resolution of 4 cm1 .
The morphology of the fractured surfaces of the starch granules
and starch foams was examined using a scanning electron microscope (SEM, Quanta 400, FEI). All starch foams were immersed in
liquid nitrogen before fracturing and were coated with a thin layer
of gold.
The thermal decomposition of the samples was measured in
a owing air atmosphere (gas ow: 100 cm3 /min) using the TA
Instruments SDT Q600 equipment in the temperature range of
30650 C at a heating rate of 10 C/min. Sample masses: 4 mg.
Sample pan type: alumina/referent pan: empty alumina.
The water adsorption capacity was determined using sample
pieces (dimensions 15 15 4 mm3 ) that had been stored at 55%
RH for 7 days before being weighed. They were then dried in an
oven at 105 C for 24 h, cooled to room temperature and weighed
immediately. The amount of adsorbed water was calculated using
Eq. (1):
Water adsorption (%) =

[(m1 m2 )/m2 ]
100

(1)

where m1 is the mass of sample before and m2 is the mass of sample

after drying. All measurements were repeated three times.
3. Results and discussion
3.1. Characterization of the native cassava starch granules and
citric acid modied cassava starch granules
The FT-IR spectrum of the NS, citric acid and their derivative
CNS are presented in Fig. 1. The spectrum of the native cassava
starch granules showed the bands typical for native cassava starch
(Kaewtatip & Tanrattanakul, 2008; Lomeli-Ramirez et al., 2014;
Riyajan, Sukhlaaied, & Keawmang, 2015). The bands observed in
the spectrum of the native starch were still present in the spectrum of the citric acid modied starch, but with a signicantly

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109

Fig. 2. SEM micrographs of native cassava starch granules (a) and citric acid modied cassava starch granules (b).

lower intensity. In addition, a new band appeared at 1732 cm1

in the spectrum of the CNS. This band was related to the esterication reaction between the carboxyl groups of citric acid and
the free hydroxyl groups of starch and belongs to C O stretching
(Fang, Fowler, Tomkinson, & Hill, 2002; Ma, Jian, Chang, & Yu, 2008;
Wilpiszewska & Czech, 2014). In the spectrum of CNS the decrease
in the band intensities for the hydroxyl groups (above 3000 cm1 ),
C H (2930 cm1 ) and the C O (12001000 cm1 ) bonds and the
bonded water molecules (15001300 cm1 ) was due to the rearrangements and formation of new hydrogen bonds in the citric acid
starch derivative.
3.2. Morphology of the starch granules and foams
The morphology of the native cassava starch and citric acid modied cassava starch granules is presented in Fig. 2. As can be seen,

the morphology of citric acid modied cassava starch was very similar to that of the natural starch granules which means that the
reaction did not affect the morphology of the granules. A similar
result was obtained by Uslu and Poat (2012) and Ma et al. (2009).
The SEM micrographs of cross-sections of the NS and CNS starch
foams and the blended starch foam with a CNS/NS ratio of 50/50 are
presented in Fig. 3. It was found that the cells formed were open
and there was a connectivity between cells. Moreover, all three
starch foams had a sandwich-type structure that was composed
of two layers. The outer layers had a smaller cell size but a more
dense structure, whereas the interior had a larger cell size and a
more expanded structure. However, the cell size and thickness of
cell walls of the native and the blended starch foams were different. As shown in Fig. 3(a), the SEM micrograph of the cross-section
of the NS foam showed a thinner cell wall with a broad distribution of cell sizes. The SEM micrographs of cross-sections of CNS

Fig. 3. SEM micrograph of cross-sections of NS foam (a), CNS foam (b) and blended starch foam with NS/CNS ratio of 50/50 (c).

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Fig. 4. The change of thickness as a function of the NS/CNS ratios.

Fig. 5. The change of density as a function of the NS/CNS ratios.

foam, Fig. 3(b), revealed a smaller cell size and a more dense structure. This change in cell size and density in the CNS foam could
be explained by the decreased chain mobility in the cross-linked
starch chains that resulted in a decreased expansion of the batter. Soykeabkaew, Supaphol, and Rujiravanit (2004) also reported
that the high viscosity of the starch caused the batter to be less
expandable, which resulted in a material with a smaller mean cell
size and a higher density. Fig. 3(c) presents the SEM micrograph
of cross-sections of the blended starch foam with a NS/CNS ratio
of 50/50. It was observed that the blended starch foam exhibited a
narrower distribution of cell sizes and thicker cell walls than in the
NS and CNS foams. This nding is in agreement with the differences
in the paste viscosities of the NS, CNS and blended starch batters
and is consistent with the data of Obanni and Bemiller (1997). These
authors reported that the pasting behavior and thermal properties
of the starch blends were special characteristics, thus the properties of starch blend batter did not resemble those of the two
components. This behavior has been also reported by other authors
(Ashogbon, 2014; Hussain, Alamri, & Mohamed, 2013).
Fig. 6. The change in water absorptivity as a function of the NS/CNS ratios.

3.3. Physical properties of the starch foams

The ratio of the two starch components had a signicant inuence on the thickness of the blended starch foams (Fig. 4). When
the ratio of the CNS increased, the thickness of the starch foam
decreased. It was clearly observed that the thickness of the NS foam,
the blended starch foam with NS/CNS ratio of 50/50 and the CNS
foam (Fig. 3) were signicantly different with average values of 3.7,
3.6 and 2.7 mm, respectively. The highest thickness in the NS foam
might be attributed to the low viscosity of the batter that reduced
the foaming ability of the starch paste.
Density is one of the very important physical properties for
practical applicability of the foams. Moreover, it is known that the
density of the foams is inversely proportional to its expansion ability (Kaisangsri, Kerdchoechuen, & Laohakunjit, 2014). In Fig. 5 the
change in density of the NS, CNS and blended starch foams is presented as a function of their composition. The density of the NS
foam (0.21 g/cm3 ) was signicantly lower than the density of the
CNS foam (0.34 g/cm3 ). This result is consistent with the SEM micrograph results (Fig. 3): the larger cell size in the NS foam refers to a
more expansible foam material compared with the CNS foam, due
to the low viscosity of the NS foam batter. The density data for NS
foam, CNS foam and the blended starch foams are in the same range
as in the starch foams prepared from corn starch cross-linked with

glyoxal (0.270.36 g/cm3 ) (Uslu & Polat, 2012). On the basis of the
density of the NS and CNS it was expected that the blend foam
density would decrease with an increase in the NS/CNS ratio. However, the change in density with the composition was not really so
straightforward. In the NS/CNS composition range from 100/0 to
40/60 a small decrease in the density was observed. The lowest density belonged to the foam with a 40/60 NS/CNS ratio (0.19 g/cm3 ).
Above this ratio with an increase of the CNS in the blend, the density of the blended starch foams seemed to increase rapidly. The
thickness and density results are in agreement with the differences in the paste viscosities of the NS, CNS and blended starch
batters (Shogren, Lawton, Doane, & Tiefenbacher, 1998). It was of
interest that, the densities of the NS/CNS blended starch foams
were lower than those in the starch foams produced with natural ber, protein, palm oil or organically modied montmorillonite
(Kaisangsri et al., 2014; Matsuda, Verceheze, Carvalho, Yamashita,
& Mali, 2013; Mello & Mali, 2014).
3.4. Water adsorption properties of the starch foams
The water adsorption test was carried out in order to determine the behavior of the starch foams when in contact with free
water. The dependence of the water absorptivity on the foam

K. Pornsuksomboon et al. / Carbohydrate Polymers 136 (2016) 107112

111

Fig. 7. TG and DTG curves of NS foam and the blended starch foam with a NS/CNS ratio of 50/50 in air.

composition is presented in Fig. 6. The NS foam showed the highest

water absorption (about 14%). A relatively high water absorptivity was expected in the native starch that had abundant hydroxyl
groups that preferred to form hydrogen bonds with water (Ayana,
Suin, & Khatua, 2014). In contrast, the water absorptivity of the
CNS foam was about half that of the NS foam and indicated that
the availability of free hydroxyl groups had decreased as a consequence of their substitution with hydrophobic ester groups in
the citric acid modied starch foams (Ayana et al., 2014; Ma et al.,
2009). It was of interest that the amount of water in all the blended
starch foams ranged from 4.7 to 6.6% which was lower than those in
the NS and CNS foams. The lower water content in the foam blends
might be related to the strong interactions between the NS and
CNS chains (Jiugao, Ning, & Xiaofei, 2005) and this prevented the
water molecules from penetrating into the blended starch foams
(Ghanbarzadeh et al., 2011; Matsuda et al., 2013).
3.5. Thermal properties of the starch foams
In Fig. 7 the thermogravimetric (TG) and the derivative thermogravimetric (DTG) curves of the native and blended starch foams
with 50/50 NS/CNS ratio are presented. The course of the decomposition was similar for both foams. In the rst step up to about 200 C
the evaporation of the adsorbed and structural water took place in
accordance with data in the literature (Kaewtatip & Tanrattanakul,
2008; Lomeli-Ramirez et al., 2014). The mass loss to 210 C was
somewhat higher in the NS than in the 50/50 NS/CNS blend foam
(6.8% and 4.9% respectively). Above 240 C the decomposition of
the starch material occurred with the onset temperatures of 247 C
for the NS/CNS blend and 290 C for NS. The lower thermal stability of the blended foam is most probably due to the lower
thermal stability of the ester bonds (Ma et al., 2009). While the
NS foam decomposed completely up to about 520 C, the decomposition of the NS/CNS blend to this temperature was only partial
even in a owing air atmosphere. This can be explained by the
stabilizing effect of the higher degree of cross-linking in the citric acid modied starch. The thermal data are in agreement with
the physical properties of the starch foams. Namely, not only the
penetration of water molecules into the foam blends is hindered,
their evaporation is also restricted. The water evaporation from the

blend foam takes place at a low, steady rate up to the decomposition temperature of the starch material, while from the native
starch foam most of the water is evaporated to 150 C. Despite
the fact that the thermal stability of the NS/CNS blend is lower by
about 40 C, the rate of the decomposition was signicantly lower
compared to the decomposition rate of the NS. The lower decomposition rate refers to stronger interactions in the blend. These
interactions are present even at higher temperatures, so while the
decomposition of native starch foam is completed above 500 C,
the residue of the blended foam at this temperature amounts about
18% and its decomposition is still in progress though at a very slow
rate.

4. Conclusions
The work was successful in being able to produce novel starch
foams by blending native cassava starch and citric acid modied
cassava starch using a baking process with properties good enough
for tray production to replace most trays produced from petroleumbased foams. The CNS foam had a high density, low thickness and
a more dense structure due to the higher viscosity of the batter,
whereas the NS foam was is more expandable because of the low
viscosity of the of NS batter. The blended starch foam with a 50/50
NS/CNS ratio revealed a uniform distribution of cell sizes with thinner cell walls than both the NS and CNS foams. The differences
in morphology, thickness and density of the starch foams may be
attributed to the different viscosity of the NS, CNS and blended
starch batters. The optimum NS/CNS ratio, that provided the lowest
density (0.19 g/cm3 ) and water adsorption capacity (4.67%) was at
the 40/60 NS to CNS ratio. While the thermal stability of the blended
starch foam was somewhat lower, the rate of water evaporation
and the decomposition rate of the starch material were signicantly slower for the citric acid modied cassava starch. These
observations are in agreement with the supposition of cross-linking
between NS and CNS chains and strong hydrogen bonds formation
in the blended NS/CNS starch foams. Thus baked foams from native
cassava starch and citric acid modied cassava starch blends could
be used to replace most trays produced from petroleum-based
foams.

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K. Pornsuksomboon et al. / Carbohydrate Polymers 136 (2016) 107112

Acknowledgements
This work was supported by the budget revenue of Prince of
Songkla University (SCI560474S). We thank Siam Modied Starch
Co., Ltd. for the native cassava starch. This paper was supported
by the Ministry of Education, Science and Technological Development, Republic of Serbia; contract grant numbers: III 45022 and
ON 172014. Thanks to Dr. Brian Hodgson for assistance with the
English.
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